CN110676469B - Carbon-supported platinum-based nanomaterial - Google Patents
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- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
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Abstract
The invention provides a carbon-supported platinum-based nanomaterial for a catalyst of a methanol fuel cell, wherein the carbon-supported platinum-based nanomaterial comprises a carbon-supported material and a platinum-based material, the platinum-based material comprises platinum and a single metal, and the single metal is iron or gold; when the single metal is iron, the mass ratio of platinum to iron is 1: 1/40; when the single metal is gold, the mass ratio of platinum to gold is 1: 1/2.
Description
Technical Field
The invention relates to a carbon-supported platinum-based nanomaterial, in particular to a carbon-supported platinum-based nanomaterial for a methanol fuel cell.
Background
The methanol fuel cell is a novel cell, and has the advantages of low fuel price, low toxicity, room temperature liquid state, small size, portability, easy storage and the like, so that the methanol fuel cell is attracted by attention. At present, the commercial methanol fuel cell catalytic material with the optimal electrocatalytic performance is a platinum group material, wherein a platinum group catalyst loaded by platinum black and high-dispersion carbon black is a hot spot for research, application and development of fuel cell catalysts. However, in practical application, the problems of cost, efficiency, stability and the like of the platinum group catalyst limit the application of the platinum group catalyst, and the development of a catalyst with high catalytic efficiency and stable performance is a problem to be solved urgently in the current methanol fuel cell. In the series developed and improved platinum-based nano catalytic materials, a binary platinum-based metal nano material consisting of two different metal elements becomes a new material which is of great interest. In most cases, binary metal nanoparticles are widely used in optical, biological and catalytic applications and exhibit excellent performance due to the synergistic effect between metals that greatly improves their physicochemical properties.
Disclosure of Invention
The invention provides a binary platinum-based metal nano material which shows better methanol catalytic activity and stability.
The invention is realized by the following steps:
a carbon-supported platinum-based nanomaterial for a catalyst of a methanol fuel cell, wherein the carbon-supported platinum-based nanomaterial comprises a carbon-supported material and a platinum-based material, the platinum-based material comprises platinum and a single metal, and the single metal is iron or gold; when the single metal is iron, the mass ratio of platinum to iron is 1: 1/40; when the single metal is gold, the mass ratio of platinum to gold is 1: 1/2.
As a further improvement, the size of the carbon particles ranges from 20 to 50 nm.
As a further improvement, the single metal is iron and the platinum particles are less than 10nm in diameter.
As a further improvement, the single metal is gold, and the diameter of the platinum particles is less than 10 nm.
The invention has the beneficial effects that: compared with a single carbon-supported platinum metal nano material, the carbon-supported platinum nano material with the platinum-iron ratio of 1:1/40 and the carbon-supported platinum nano material with the platinum-gold ratio of 1:1/2 have higher electro-catalytic performance on methanol and higher stability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a scanning electron microscope image of a carbon-supported platinum nanomaterial provided by the present invention.
FIG. 2 is a scanning electron microscope image of the carbon-supported platinum nanomaterial provided by the invention.
FIG. 3 shows that the carbon-supported platinum nano-material catalyst with different platinum-iron ratios provided by the invention is 0.5mol/L H2SO4+0.5mol/L CH3Cyclic voltage in OH solutionAnd (6) installing a picture.
FIG. 4 shows that the carbon-supported platinum nano-material catalyst with different platinum-iron ratios provided by the invention is 0.5M H2SO4The solution was purged with nitrogen and subjected to cyclic voltammogram.
FIG. 5 shows that the carbon-supported platinum nanomaterial catalyst with different platinum-iron ratios provided by the invention is used at 0.5MH2SO4And (3) introducing oxygen into the solution to obtain a cyclic voltammogram.
FIG. 6 shows that the carbon-supported platinum nano-material catalyst with different platinum ratios is 0.5mol/LH2SO4+0.5mol/L CH3Cyclic voltammograms in OH solution.
FIG. 7 shows that the carbon-supported platinum nano-material catalyst with different platinum ratios provided by the invention is 0.5M H2SO4The solution was purged with nitrogen and subjected to cyclic voltammogram.
FIG. 8 shows that the carbon-supported platinum nano-material catalyst with different platinum ratios provided by the invention is 0.5M H2SO4And (3) introducing oxygen into the solution to obtain a cyclic voltammogram.
FIG. 9 shows that the carbon-supported platinum nano-material catalyst with different platinum-iron ratios provided by the invention is 0.5M H2SO4+0.5MCH3The electrocatalytic performance in OH solution stabilizes the curve.
FIG. 10 shows that the carbon-supported platinum nanomaterial catalysts with different platinum ratios provided by the present invention are 0.5M H2SO4+0.5M CH3Stable electrocatalytic performance curve in OH solution.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The invention provides a carbon-supported platinum-based nanomaterial, which comprises a carbon-supported nanomaterial and a platinum-based nanomaterial, wherein the platinum-based nanomaterial comprises platinum and a single metal. The single metal may be iron or gold. When the single metal is iron, the mass ratio of the platinum to the iron is preferably 1: 1/40; when the single metal is gold, the mass ratio of platinum to gold is preferably 1: 1/2.
The carbon supporting material is round or oval carbon particles. The size of the carbon particles is in the range of 20-50 nm. When the single metal is iron, the diameter of the platinum particles is less than 10nm, and the iron is a doped metal. When the single metal is gold, the diameter of the platinum particles is less than 10nm, and the gold is one of the main components of the platinum nano material.
The carbon-supported platinum-based nano material is prepared by a hydrothermal synthesis method. When the single metal is iron, the carbon-supported platinum-based nano material is a carbon-supported platinum nano material, and the iron is a doped metal; when the single metal is gold, the carbon-supported platinum-based nano material is a carbon-supported platinum nano material, and gold is one of main components of the platinum nano material.
The preparation process of the carbon-supported platinum nano material comprises the following steps: dissolving 100mg trisodium citrate dihydrate by using 1mL of water, adding 10mL of ethylene glycol, shaking up, adding potassium chloroplatinate and ferric chloride according to a certain proportion, mixing uniformly, adding 10mg of carbon powder, performing ultrasonic treatment for 30min by using an ultrasonic cleaner, taking out, putting into a vacuum drier, reducing pressure, degassing, adjusting the pH value to 10 by using a 2% NaOH solution, transferring the solution to a hydrothermal synthesis reaction kettle, and reacting for 4 hours at 120 ℃. After the reaction is finished, the sample is subjected to suction filtration, ethanol cleaning and low-temperature drying to obtain the carbon-supported platinum nano-materials with different platinum-iron ratios, as shown in table 1. Referring to FIG. 1, (A), (B), (C) and (D) are SEM images of the samples in Table 1, wherein the spherical or ellipsoidal particles with a diameter of 20-50nm in the 4 segments of (A), (B), (C) and (D) are carbon-supported materials. In the sample (a), it was clearly observed that platinum particles having a series of diameters of less than 10nm were supported on the surface of the carbon support, wherein the platinum particles were in a state of dispersion and a small portion of the particles were agglomerated; in samples (B), (C) and (D), a large number of platinum particles smaller than 10nm were supported on the surface of the carbon support in an agglomerated or a small-part dispersed form, and the increase in the iron content did not change the shape, size and supporting amount of the platinum particles to a large extent.
TABLE 1 carbon-supported platinum nanomaterials with different platinum-iron ratios
| Sample numbering | Platinum iron ratio | Content of platinum/%) | Iron content/%) |
| (A)C-Pt-1 | 1:0 | 20 | 0 |
| (B)C-Pt-2 | 1:1/80 | 20 | 0.25 |
| (C)C-Pt-3 | 1:1/40 | 20 | 0.5 |
| (D)C-Pt-4 | 1:1/8 | 20 | 2.5 |
The preparation process of the carbon-supported platinum nano material comprises the following steps: dissolving 100mg trisodium citrate dihydrate by using 1mL of water, adding 10mL of ethylene glycol, shaking up, adding potassium chloroplatinate and chloroauric acid in a certain proportion, mixing uniformly, adding 10mg of carbon powder, performing ultrasonic treatment for 30min by using an ultrasonic cleaner, taking out, putting into a vacuum drier, reducing pressure, degassing, adjusting the pH value to 10 by using a 2% NaOH solution, transferring the solution to a hydrothermal synthesis reaction kettle, and reacting for 4 hours at 120 ℃. After the reaction is finished, the sample is subjected to suction filtration, ethanol cleaning and low-temperature drying to obtain the carbon-supported platinum nano-materials with different platinum proportions, as shown in Table 2. Referring to FIG. 2, (A), (B), (C) and (D) are SEM images of the samples in Table 2, wherein the spherical or ellipsoidal particles with a diameter of 20-50nm in the 4 segments of (A), (B), (C) and (D) are carbon-supported materials. In samples (a) (C) (D), it was observed that platinum particles having a diameter of less than 10nm agglomerated or a small portion of platinum ions supported on the surface of the carbon carrier were present in the form of a plurality of platinum particles having a diameter of less than 10nm dispersed or a small portion of platinum ions supported on the surface of the carbon carrier were present in the form of particles having a diameter of less than 20nm agglomerated or a small portion of platinum ions was present in the sample (B). In the platinum nano material, the change of the gold content changes the dispersion form of the nano particles to a certain extent.
TABLE 2 carbon-supported platinum nano-materials of different platinum proportions
| Sample numbering | Platinum proportion | Content of platinum/%) | Content of gold/%) |
| (A)C-Pt-Au-1 | 1:1/4 | 20 | 5 |
| (B)C-Pt-Au-2 | 1:1/2 | 20 | 10 |
| (C)C-Pt-Au-3 | 1:1 | 20 | 20 |
| (D)C-Pt-Au-4 | 1:2 | 20 | 40 |
The carbon-supported platinum-based nanomaterial provided by the invention is a catalyst for a methanol fuel cell. To illustrate the effect of carbon-supported platinum-based nanomaterials on the electrocatalytic properties of methanol, electrochemical tests were performed on the samples in tables 1 and 2, respectively.
The step of electrochemically testing the sample comprises: 2mg of the sample was dispersed in 0.5mL of anhydrous ethyl acetateAdding 10uLNafion solution into alcohol, and putting into an ultrasonic cleaner for ultrasonic treatment for 30-60min to form a uniform suspension. Dripping 10uL of suspension solution on the surface of a polished glassy carbon electrode with the diameter of 5mm, and volatilizing the solvent for later use; taking a graphite electrode as a counter electrode, a saturated calomel electrode as a reference electrode and a platinum-based nano material electrode as a working electrode at the concentration of 0.5mol/L H2SO4Electrochemical testing of samples was performed in solution systems that were acidic media.
Referring to FIG. 3, the ratio of Pt to Fe is 0.5mol/L H2SO4+0.5mol/L CH3The scanning speed of the cyclic voltammogram in the OH solution is 0.05V/s. As can be seen from the figure, when the potential is swept forward, an oxidation peak of methanol appears near 0.65V; the peak appearing around 0.44V at the negative potential sweep is the intermediate product COadAn oxidation peak; the current intensity of the methanol oxidation peak is increased along with the increase of the Fe content, the current intensity of the methanol oxidation peak reaches the maximum when the platinum-iron ratio reaches 1:1/40, and the current intensity is slightly increased compared with a sample with the platinum-iron ratio of 1:1/80, namely the increasing benefit of the continuous increase of the platinum-iron ratio on the current intensity of the methanol oxidation peak is poor under the condition; when the platinum-iron ratio reached 1:1/8, the methanol oxidation peak amperage was already significantly lower than the carbon-supported platinum sample with zero iron content. Referring to FIGS. 4 and 5, the carbon-supported platinum nanomaterial catalyst with different Pt/Fe ratios was found to be 0.5M H2SO4And respectively introducing nitrogen and oxygen into the solution to obtain a cyclic voltammogram. When the system is filled with nitrogen (figure 4), it can be observed that the increase of the iron content leads to the enhancement of the hydrogen desorption signal (-0.2V-0.0V) of the carbon-supported platinum nano material; the electrochemical active surface area of the catalyst can be calculated according to the absorption and desorption areas of hydrogen, and therefore, the increase of the iron content can be inferred to increase the electrochemical active surface area of the carbon-supported platinum nano material. The conclusion is verified from the negative-going scan of the electrochemical curve in fig. 4 for the platinum metal surface oxygen reduction signal at the potential range of 0.3-0.7V; when the iron content is increased, the oxygen reduction signal on the surface of the platinum metal becomes stronger, and when the platinum-iron ratio is 1:1/40, the signal reaches the maximum, namely the electrochemical active surface area of the sample under the condition is the maximum. When systemWhen oxygen is introduced (fig. 5), the catalytic activity of the carbon-supported platinum can be judged from the change of the oxygen reduction peak potential on the platinum metal surface; when the content of iron is increased, the oxygen reduction peak potential on the surface of the platinum metal is obviously shifted positively, wherein when the ratio of the platinum to the iron is 1:1/40, the initial potential of the oxygen reduction peak on the surface of the platinum metal is the minimum in negative scanning, namely the electrocatalytic activity of the sample under the condition is optimal.
Referring to FIG. 6, the carbon-supported platinum nano-material catalysts with different platinum ratios are shown at 0.5mol/L H2SO4+0.5mol/L CH3The scanning speed of the cyclic voltammogram in the OH solution is 0.05V/s. As can be seen from the graph, the current intensity of the methanol oxidation peak increases and then decreases as the gold content increases, and reaches the maximum when the platinum-gold ratio is 1: 1/2. Referring to FIGS. 7 and 8, the carbon-supported Pt/Au nanomaterial catalyst with different Pt ratios is shown at 0.5M H2SO4And respectively introducing nitrogen and oxygen into the solution to obtain a cyclic voltammogram. When nitrogen is introduced into the system (fig. 7), it can be observed that, as the gold content increases, the hydrogen desorption signal (-0.2V-0.0V) and the oxygen reduction signal (0.3V-0.7V) of the platinum-gold-supported carbon nano material are increased and then decreased; the signal is maximal when the platinum-gold ratio is 1:1/2, i.e. the electrochemically active surface area of the sample is maximal under this condition. When oxygen is introduced into the system (figure 8), as the content of gold is increased, particularly the ratio of platinum to gold is increased from 1:1/2 to 1:2, the oxygen reduction peak potential on the surface of the platinum metal is not obviously changed, so that the catalytic capability of the carbon-supported platinum to methanol is enhanced mainly through the increase of the electrochemical active area of the platinum.
Referring to FIG. 9, the carbon-supported Pt nanomaterial catalyst with different Pt/Fe ratios is shown at 0.5M H2SO4+0.5MCH3The electrocatalytic performance stability curve in OH solution is that the ratio of carbon-loaded platinum nano material catalyst to different platinum and iron is 0.5mol/L H2SO4+0.5mol/L CH3And performing cyclic voltammetry test in an OH solution, wherein the scanning potential range is-0.2V-1.1V, the scanning speed is 0.05V/s, and the current intensity under the potential condition of 0.65V of a methanol oxidation peak is used for plotting the cycle number. As can be seen from the figure, when the iron content is zero, the carbon-supported platinum nano-material is stillHowever, the catalytic performance is not ideal enough but relatively stable electrocatalytic performance is maintained, and signals of the platinum nano material catalyst synthesized under different platinum-iron proportion conditions are enhanced to a certain extent along with the increase of the cycle number and then are attenuated to different degrees; the signal enhancement can be attributed to the cleaning and activation of the electrochemically active surface of the catalyst in the acidic medium under the cyclic test condition as the cycle number is increased; the carbon-supported platinum nanomaterial catalyst with the platinum-iron ratio of 1:1/40 still maintains high catalytic activity after 1000 cycles.
Referring to FIG. 10, the carbon-supported platinum nano-material catalyst with different platinum ratios is shown at 0.5M H2SO4+0.5MCH3The electrocatalytic performance stability curve in OH solution is that the ratio of carbon-loaded platinum nano material catalyst to platinum is 0.5mol/L H2SO4+0.5mol/L CH3And performing cyclic voltammetry test in an OH solution, wherein the scanning potential range is-0.2V-1.1V, the scanning speed is 0.05V/s, and the current intensity under the potential condition of 0.65V of a methanol oxidation peak is used for plotting the cycle number. It can be seen from the figure that except the platinum nanomaterial catalyst with the platinum ratio of 1:1/2, the catalysts with other platinum ratios have larger signal attenuation after 400 cycles of cycle test, and the performance is obviously lower than that of the platinum nanomaterial catalyst with zero iron content in fig. 9; and the platinum nano material catalyst with the platinum ratio of 1:1/2 still maintains higher catalytic activity after 1000 cycles of cycle test.
The carbon-loaded platinum-based nano material provided by the invention has the following advantages: the carbon-supported platinum nano material with the platinum-iron ratio of 1:1/40 and the carbon-supported platinum nano material with the platinum-gold ratio of 1:1/2 both have high electrocatalytic performance on methanol and high stability.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A carbon-supported platinum-based nanomaterial for a catalyst of a methanol fuel cell, wherein the carbon-supported platinum-based nanomaterial comprises a carbon-supported material and a platinum-based material, the platinum-based material comprises platinum and a single metal, and the single metal is iron or gold; when the single metal is iron, the mass ratio of platinum to iron is 1: 1/40; when the single metal is gold, the mass ratio of the platinum to the gold is 1: 1/2; the carbon load material is carbon powder; the carbon-supported platinum-based nano material is prepared by a hydrothermal synthesis method.
2. The carbon-supported platinum-based nanomaterial of claim 1, wherein the carbon-supported material is round or oval carbon particles.
3. The carbon-supported platinum-based nanomaterial of claim 2, wherein the size of the carbon particles is in the range of 20nm to 50 nm.
4. The carbon-supported platinum-based nanomaterial of claim 1, wherein the single metal is iron and the platinum particles have a diameter of less than 10 nm.
5. The carbon-supported platinum-based nanomaterial of claim 1, wherein the single metal is gold and the platinum particles have a diameter of less than 10 nm.
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| CN107293757A (en) * | 2017-07-05 | 2017-10-24 | 西南大学 | The preparation method of PtCoFe/WC C oxygen reduction catalysts |
| CN109935847A (en) * | 2017-12-15 | 2019-06-25 | 中国科学院大连化学物理研究所 | A kind of preparation method of the loaded platinum base alloy catalyst of low-temperature fuel cell |
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